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HRID 1284596作成日:2026年10月25日

Toluene → 2-Benzothiazolamine, 4-chloro-

https://huagongshe.com/reaction/1284596

反応式

関与物質

役割名称HCID仕込み量
反応物TolueneHCID 1140—
反応物Sodium CarbonateHCID 10340—
反応物Sulfuryl chlorideHCID 24648—
反応物N-(2-Chlorophenyl)thioureaHCID 737139—
溶媒ChlorobenzeneHCID 7964—
生成物2-Benzothiazolamine, 4-chloro-HCID 29872—

反応条件

温度20 °C

反応手順

210 Parts of sulfuryl chloride were added within about 2 hours at a temperature of 35°-40° C. to a stirred mixture of 186.5 parts of 2-chlorophenylthiourea, 500 parts of toluene, 300 parts of chlorobenzene and 11 parts of sodium carbonate. The gas development being terminated, 250 parts of water were added, the solvent mixture was distilled off with steam, and the remaining aqueous phase was combined with 500 parts of 30% hydrochloric acid. Filtration from the undissolved matter was carried out at about 90° C., the filtrate was cooled to about 20° C., and the free amine was precipitated from the 2-amino-4-chlorobenzothiazole dissolved as hydrochloride by adding excess sodium hydroxide solution until a final pH of 8.5-9.0 was adjusted. The product was suction-filtered, washed to neutral with water, and dried. 170 Parts of 2-amino-4-chlorobenzothiazole having a melting point of 199°-200° C. (92.4% of th.) were obtained.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04563533
出典データセットuspto-grants-1986_01
ORD IDord-6a0536c46e974e7b82e86074f93bb4ff
出典メモuspto-grants-1986_01